The exchange bias effect has been studied in Ni/ NiO nanogranular samples prepared by mechanical milling and partial hydrogen reduction of NiO; the Ni weight fraction varied between 4% and 69%. In this procedure, coarse-grained NiO powder has been ball milled in air for 20 h and subsequently subjected to annealing in H 2 ͑at a temperature ranging between 200 and 300°C͒ to induce the formation of metallic Ni. The structural properties of the samples have been studied by x-ray diffraction, electron microscopy, and extended x-ray absorption fine structure. The magnetic properties have been extensively investigated by carrying out hysteresis loops and magnetization measurements in the 5 -300 K temperature range, in zero-field-cooling and fieldcooling conditions. The results indicate that both in the as-milled NiO powder and in the hydrogenated samples, the NiO phase is composed of nanocrystallites ͑having a mean size of ϳ20 nm, structurally and magnetically ordered͒ and of highly disordered regions. The samples with low Ni content ͑up to 15%͒ can be modeled as a collection of Ni nanoparticles ͑mean size of ϳ10 nm͒ dispersed in the NiO phase; with increasing Ni content, the Ni nanoparticles slightly increase in size and tend to arrange in agglomerates. In the Ni/ NiO samples, the exchange field depends on the Ni amount, being maximum ͑ϳ600 Oe͒, at T = 5 K, in the sample with 15% Ni. However, exchange bias is observed also in the as-milled NiO powder, despite the absence of metallic Ni. In all the samples, the exchange bias effect vanishes at ϳ200 K. We propose a mechanism for the phenomenon based on the key role of the disordered NiO component, showing a glassy magnetic character. The exchange bias effect is originated by the exchange interaction between the Ni ferromagnetic moments and the spins of the disordered NiO component ͑in the as-milled NiO powder, the existence of ferromagnetic moments has been connected to chemical inhomogeneities of the NiO phase͒. The thermal dependence of the exchange bias effect reflects the variation of the anisotropy of the NiO disordered component with temperature.

No abstract

Pure, crystalline, ∼10 nm lithium ferrite phase (Li0.5Fe2.5O4), was successfully synthesized at very low temperature using a modified combustion method. The crystal structure and microstructure evolution of this system upon annealing were monitored by a careful investigation of X-ray diffractograms collected on a synchrotron source. Comparative analysis of the results obtained from the full profile Rietveld method (in reciprocal space) and the pair distribution function method (in direct space) was carried out. Nanocrystalline samples exhibit similar crystal structure, on average, with a partial ordering of Li+ and Fe3+ ions between octahedral 4b and 12d sites on the spinel crystal lattice (space group P4332). After annealing at 973 K, cation distribution changes to a completely ordered, resembling that which is seen in the bulk lithium ferrite. The PDF analysis reveals abnormally high values of oxygen atomic displacement parameters in tetrahedral 8c sites (O1) indicating a significant disordering of the O1 network and suggests migration of lithium ions from 4b sites to the outer layers of nanoparticles. Analysis of room temperature Mössbauer spectra has shown that the hyperfine field for Fe3+ ions in tetrahedral 8c sites is the most sensitive on increasing the particle size and improving the crystallinity. From the differential thermal analysis, it was found that a lower driving force is required to induce an order−disorder phase transition in nanocrysalline samples, compared to the bulk-like sample, presumably due to the higher crystal disordering in these samples.

No abstract

No abstract

No abstract

No abstract

No abstract